CN114487010A - Method for evaluating heated cigarette formula based on change of heating energy of substance - Google Patents
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- CN114487010A CN114487010A CN202210137148.4A CN202210137148A CN114487010A CN 114487010 A CN114487010 A CN 114487010A CN 202210137148 A CN202210137148 A CN 202210137148A CN 114487010 A CN114487010 A CN 114487010A
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- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 60
- 238000000034 method Methods 0.000 title claims abstract description 35
- 238000010438 heat treatment Methods 0.000 title claims abstract description 19
- 239000000126 substance Substances 0.000 title claims abstract description 16
- 230000008859 change Effects 0.000 title claims abstract description 10
- 238000009472 formulation Methods 0.000 claims abstract description 20
- 239000000203 mixture Substances 0.000 claims abstract description 20
- 238000011156 evaluation Methods 0.000 claims abstract description 9
- 238000002474 experimental method Methods 0.000 claims abstract description 6
- 238000001595 flow curve Methods 0.000 claims description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- 238000012360 testing method Methods 0.000 claims description 4
- 238000004364 calculation method Methods 0.000 claims description 3
- 230000000630 rising effect Effects 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- 238000002411 thermogravimetry Methods 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 230000001953 sensory effect Effects 0.000 abstract description 6
- 238000012512 characterization method Methods 0.000 abstract description 3
- 230000035945 sensitivity Effects 0.000 abstract description 2
- 241000208125 Nicotiana Species 0.000 description 10
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- 238000012546 transfer Methods 0.000 description 7
- 230000000391 smoking effect Effects 0.000 description 6
- 239000000779 smoke Substances 0.000 description 5
- 238000002485 combustion reaction Methods 0.000 description 4
- 238000000113 differential scanning calorimetry Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000001938 differential scanning calorimetry curve Methods 0.000 description 3
- 238000012423 maintenance Methods 0.000 description 3
- 239000000443 aerosol Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 238000010587 phase diagram Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 235000019505 tobacco product Nutrition 0.000 description 2
- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000004069 differentiation Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 238000013178 mathematical model Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 210000000214 mouth Anatomy 0.000 description 1
- 229960002715 nicotine Drugs 0.000 description 1
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000002076 thermal analysis method Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P90/00—Enabling technologies with a potential contribution to greenhouse gas [GHG] emissions mitigation
- Y02P90/30—Computing systems specially adapted for manufacturing
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- General Health & Medical Sciences (AREA)
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Abstract
The invention discloses a method for evaluating a heated cigarette formula based on the change of heating energy of a substance, which comprises the following steps: (1) preparing a plurality of heated cigarette formula samples and standard formula samples; (2) heat flow experiment; (3) calculating the curve similarity of a plurality of heated cigarette formulas and a standard formula; (4) evaluation of multiple heated cigarette formulations. The method avoids subjective factor influence and difference characterization brought by the traditional method of artificial sensory evaluation, and is more objective and efficient, good in repeatability, high in sensitivity and simple to operate.
Description
Technical Field
The invention belongs to the technical field of tobacco, and particularly relates to a method for evaluating a heated cigarette formula based on the change of the heating energy of a substance.
Background
A heating cigarette, also known as a heating non-combustible cigarette product, is a novel tobacco product which meets the requirements of smokers by heating tobacco materials through a heating source and volatilizing nicotine and flavor substances in the tobacco materials to generate smoke. Different from the traditional cigarette, the cigarette is heated without combustion, and the smoke generation and transmission mechanism is completely changed, so that the harmful components generated by high-temperature combustion and pyrolysis of tobacco are effectively reduced.
The aerosol source of the traditional cigarette is mainly combustion and pyrolysis of tobacco leaves. Different from the traditional cigarette, the cigarette heating does not have the problem of high-temperature combustion of tobacco, and the smoke generation and transfer mechanism of the cigarette heating is greatly different from that of the traditional cigarette. In a mixed system containing two or more components, a process of transferring a certain component or components from a high concentration region to a low concentration region due to a concentration difference is called a mass transfer process; the mass transfer process can be carried out in one phase or between two phases, and the mass transfer between the two phases is the basis of the separation process; mixing and transport involve changes in mass or concentration within a single phase or between phases. The heat transfer process is physically "similar" to the mass transfer process, involving changes in heat or temperature within or between phases. Whether a conventional tobacco product or a heated cigarette, its use can be described as the tobacco substrate being heated, releasing smoke material, forming an aerosol, and drawn into the oral cavity by suction. Thus, the transport-transport process of smoke substances is the core and the heating of the tobacco substrate is the basis. Differential Scanning Calorimetry (DSC) is a thermal analysis method that measures the power difference (e.g., in the form of heat) input to a sample and a reference as a function of temperature at a programmed temperature. The curve recorded by the differential scanning calorimeter is called a DSC curve, and is a curve obtained by taking the rate of heat absorption or heat release of a sample, i.e. the heat flow rate dH/dt (unit can be milliJoule per second) as an ordinate and taking the temperature T or time T as an abscissa. Differential scanning calorimetry can measure a variety of thermodynamic and kinetic parameters, such as specific heat capacity, heat of reaction, heat of transformation, phase diagram, reaction rate, crystallization rate, polymer crystallinity, sample purity, and the like. The method has the advantages of wide application temperature range (-175-725 ℃), high resolution and less sample consumption; it is suitable for analyzing inorganic matter, organic compound and medicine. It can be said that the heat flow method can be used to study the change of energy generated when the substance is heated, and each substance has its unique heat flow fingerprint curve in a strict sense.
At present, the formula maintenance of the heated cigarette mainly adopts a manual smoking evaluation method. Adopting a large number of personnel to evaluate and score the smoking of the heated cigarette core formulas of different batches, and finally obtaining the difference value between the heated cigarette formula sample and the standard formula sample; the numerical value is different from person to person, mainly depends on experience accumulation and evaluation judgment of formula personnel, and has the advantages of high working strength, strong subjectivity and obvious differentiation. In order to improve the universality of the formula maintenance of the heated cigarettes and reduce the workload of formula designers, a tobacco group formula database and a mathematical model of the heated cigarettes are established by utilizing heat flow, and the formula maintenance is assisted by utilizing objective data, so that the method has important significance for reducing the influence of subjective factors and the characterization of differences and improving the quality stability of the heated cigarettes.
The invention is therefore proposed.
Disclosure of Invention
The invention provides a method for evaluating a formula of a heated cigarette based on the change of heating energy of a substance, and particularly relates to a method for evaluating the stability of the formula of the heated cigarette based on the change of the heating energy of the substance by adopting a correlation coefficient method.
The technical scheme of the invention is as follows:
a method for evaluating a heated cigarette formula based on the change of the heating energy of a substance comprises the following steps:
(1) preparing a plurality of heated cigarette formula samples and standard formula samples;
(2) a heat flow curve is obtained through a heat flow experiment;
(3) calculating the curve similarity of a plurality of heated cigarette formulas and a standard formula;
(4) evaluation of multiple heated cigarette formulations.
Preferably, the mass of each formula sample in step (1) is not less than 5 g; before thermogravimetric experiment, the sample was equilibrated in an environment with a temperature of (22 + -1) ° C and a relative humidity of (60 + -2)% for 48 hours.
Preferably, the heat flow experiment step (2) is as follows: a differential scanning calorimeter is adopted; weighing a certain mass of the formula sample, placing the formula sample in a crucible, covering a crucible cover, compacting and sealing; the temperature rising procedure is as follows: the initial temperature was 30 deg.C, the ramp rate was 10 deg.C/min, the end temperature was 350 deg.C, and the test was conducted at a flow rate of 50mL/min air. Before the experiment, the DSC is kept for at least 10min under the condition of 900 ℃ in the air atmosphere, so that impurities in the furnace body are discharged.
Preferably, the temperature accuracy of the differential scanning calorimeter is not less than 0.1K; the enthalpy precision is not lower than 1%; the signal-to-noise ratio tested by using 4, 4' -azodiphenylmethyl ether as a standard substance is more than 30.
Preferably, the step (3) of calculating the similarity of the curves comprises the following steps: the standard formulation sample x (x)1,x2,...,xn) And heating cigarette formulation sample y (y)1,y2,...,yn) The n-dimensional heat flow curve data of (a) is calculated according to the following formula:
ρx,yi.e. the degree of similarity; wherein x isi,yi(i ═ 1,2,. and n) are the heat flow fingerprint data for the n time points for the standard and heated cigarette formula samples, respectively;
the mean values of the heat flow fingerprint data of n time points of the standard formula sample and the heated cigarette formula sample are respectively.
Preferably | ρ |x,yThe closer the | value is to 1, the smaller the quality difference between the heated cigarette formula and the standard formula is; | ρ |x,yThe closer the | value is to 0, the greater the quality difference between the heated cigarette formulation and the standard formulation. Rhox,yIs in the range of [ -1, +1]In the meantime.
The invention has the following beneficial effects:
1. the method avoids subjective factor influence and difference characterization brought by the traditional method of smoking by means of artificial sensory evaluation, improves the universality of heated cigarette formula development, reduces the workload of formula designers, and improves the stability of the quality of the heated cigarettes.
2. The method has the advantages of simple operation, small sample usage amount within 10mg, no complex pretreatment process, and direct measurement by adding the sample into an aluminum crucible. The method does not use any wet chemical means such as solvent and the like, is nontoxic and harmless, has no harm to operators, and does not cause environmental pollution.
3. The method is quick, simple and convenient, the measuring time does not exceed 40min, and the measuring cost is low. The evaluation result is more objective and efficient, the repeatability is good, the sensitivity is high, and the method has unique advantages in the development of heating cigarette products in the tobacco industry.
4. According to the method, the thermal chemical reaction models with different formulas can be established through dynamic research of DSC while providing the change information of the heated mass of the substance, more data such as specific heat capacity, reaction heat, conversion heat, phase diagram, reaction rate, activation energy, pre-index factors, reaction stages, heat and mass transfer information and the like are obtained, and a basis is provided for adapting the heated cigarette raw materials to the smoking set.
Drawings
FIG. 1 is a DSC plot of seven heated cigarette formulation samples (samples) and one standard formulation sample (standard) of example 1.
FIG. 2 is the | ρ | of seven heated cigarette formula samples (samples) and one standard formula sample (standard) of example 1x,y| a numerical map.
Detailed Description
The present invention is further illustrated by the following examples, but is not limited to these examples. The experimental methods not specified in the examples are generally commercially available according to the conventional conditions and the conditions described in the manual, or according to the general-purpose equipment, materials, reagents and the like used under the conditions recommended by the manufacturer, unless otherwise specified. The starting materials required in the following examples and comparative examples are all commercially available.
Example 1
1. Selecting 1 standard formula sample (standard sample) and 7 heated cigarette formula samples (samples) each 5g, respectively sieving with 100 mesh sieve, and balancing in constant temperature and humidity environment with a relative humidity of (60 + -2)% at (22 + -1) ° C for 48 hr.
2. Before sample analysis, a thermogravimetric analyzer is arranged and kept for 10min at 900 ℃ so as to completely discharge impurities in the furnace body, and an empty crucible is taken as a reference. Weigh (5.00 ± 0.05) mg of sample into a hot-weight platinum crucible, with the temperature program: the initial temperature was 30 deg.C, the ramp rate was 10 deg.C/min, the end temperature was 350 deg.C, and the test was conducted at a flow rate of 50mL/min air. Samples of the standard formulation and seven heated cigarette formulations were taken along with a 350 ℃ heat flow curve (DSC curve) as shown in figure 1.
3. The curve similarity of seven of the heated cigarette formulas to a standard formula is calculated according to the following formula:
wherein xi,yi(i 1, 2.. and n) are the heat flow fingerprint data of n time points of the standard formula sample (standard sample) and the heated cigarette formula sample (sample), respectively,
the mean of the heat flow fingerprint data for n time points of the standard formula sample (standard) and the heated cigarette formula sample (sample), where n is 1921, respectively. To obtain rhox,yThe numerical values, i.e., the degrees of similarity, are shown in table 1 and fig. 2.
TABLE 1 heating of cigarette formulation samples (samples) and standard formulation samples (standards) to px,yNumerical value
| | Sample | 1 | Sample 2 | Sample 3 | Sample No. 4 | Sample No. 5 | Sample No. 6 | Sample 7 | |
| |
1 | 0.949 | 0.973 | 0.892 | 0.915 | 0.922 | 0.983 | 0.942 |
As can be seen from table 1 and fig. 2, the correlation coefficient for sample 6 to the standard was closest to 1, indicating that sample 6 had the least difference in quality from the selected heated cigarette formulation.
In order to further verify the calculation results, the above-mentioned heated cigarette formula samples (samples) and standard formula samples (standards) were organized by experts for sensory smoking, and the smoking results are shown in table 2.
TABLE 2 sensory test results of the expert
| | Sample | 1 | Sample 2 | Sample 3 | Sample No. 4 | Sample No. 5 | Sample No. 6 | Sample 7 | |
| Total score | 100 | 92 | 93 | 85 | 90 | 91 | 97 | 92 | |
| Evaluation of quality Difference | - | Difference | Difference | The difference is large | Difference | Difference | Slight difference | Difference |
As can be seen from the results in table 2, the sensory difference between the heated cigarette formula sample 6 and the standard formula sample was minimal, and the sensory difference between the heated cigarette formula sample 3 and the standard formula sample was greater; consistent with the results of the above calculations. Therefore, it may be preferable to first make replacement fine adjustments to sample 6 in a heated cigarette formulation module replacement.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (6)
1. A method for evaluating a heated cigarette formula based on the change of the heating energy of a substance is characterized by comprising the following steps:
(1) preparing a plurality of heated cigarette formula samples and standard formula samples;
(2) a heat flow curve is obtained through a heat flow experiment;
(3) calculating the curve similarity of a plurality of heated cigarette formulas and a standard formula;
(4) evaluation of multiple heated cigarette formulations.
2. The method of claim 1, wherein step (1) each formulation sample has a mass of not less than 5 g; before thermogravimetric experiment, the sample was equilibrated in an environment with a temperature of (22 + -1) ° C and a relative humidity of (60 + -2)% for 48 hours.
3. The method of claim 1, wherein the heat flow experimental step (2) is: a differential scanning calorimeter is adopted; weighing a certain mass of the formula sample, placing the formula sample in a crucible, covering a crucible cover, compacting and sealing; the temperature rising procedure is as follows: the initial temperature was 30 deg.C, the ramp rate was 10 deg.C/min, the end temperature was 350 deg.C, and the test was conducted at a flow rate of 50mL/min air.
4. The method according to claim 3, characterized in that the temperature accuracy of the differential scanning calorimeter is not less than 0.1K; the enthalpy precision is not lower than 1%; the signal-to-noise ratio tested by using 4, 4' -azodiphenylmethyl ether as a standard substance is more than 30.
5. The method according to claim 1, wherein the curve similarity calculation step (3) is: the standard formulation sample x (x)1,x2,...,xn) And heating cigarette formulation sample y (y)1,y2,...,yn) The n-dimensional heat flow curve data of (a) is calculated according to the following formula:
ρx,yi.e. the degree of similarity; wherein x isi,yi(i ═ 1,2,. and n) are the heat flow fingerprint data for the n time points for the standard and heated cigarette formula samples, respectively;
the mean values of the heat flow fingerprint data of n time points of the standard formula sample and the heated cigarette formula sample are respectively.
6. The method of claim 5 wherein | ρ |, wherex,yThe closer the | value is to 1, the smaller the quality difference between the heated cigarette formula and the standard formula is; | ρ |x,yThe closer the | value is to 0, the greater the quality difference between the heated cigarette formulation and the standard formulation.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10132807A (en) * | 1996-10-29 | 1998-05-22 | Mitsubishi Rayon Co Ltd | Evaluation method for smoke of cigarette |
| CN102980913A (en) * | 2012-11-13 | 2013-03-20 | 湖北中烟工业有限责任公司 | Biological thermochemistry method for safety evaluation and screening of cigarette auxiliary material |
| CN102980912A (en) * | 2012-11-13 | 2013-03-20 | 湖北中烟工业有限责任公司 | Bio-thermo-chemical method used in cigarette flavor and fragrance security screening |
| CN104713902A (en) * | 2015-03-06 | 2015-06-17 | 云南中烟工业有限责任公司 | Method for evaluating quality of essence spice for tobaccos by using calorie value as index |
| CN108120653A (en) * | 2017-12-13 | 2018-06-05 | 安徽中烟工业有限责任公司 | A kind of method of finished cigarettes quality stability between evaluation batch |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10132807A (en) * | 1996-10-29 | 1998-05-22 | Mitsubishi Rayon Co Ltd | Evaluation method for smoke of cigarette |
| CN102980913A (en) * | 2012-11-13 | 2013-03-20 | 湖北中烟工业有限责任公司 | Biological thermochemistry method for safety evaluation and screening of cigarette auxiliary material |
| CN102980912A (en) * | 2012-11-13 | 2013-03-20 | 湖北中烟工业有限责任公司 | Bio-thermo-chemical method used in cigarette flavor and fragrance security screening |
| CN104713902A (en) * | 2015-03-06 | 2015-06-17 | 云南中烟工业有限责任公司 | Method for evaluating quality of essence spice for tobaccos by using calorie value as index |
| CN108120653A (en) * | 2017-12-13 | 2018-06-05 | 安徽中烟工业有限责任公司 | A kind of method of finished cigarettes quality stability between evaluation batch |
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